Sulfuric Acid → 6,7-Dihydro-2-methyl-4(5H) benzofuranone

HRID 1252794

반응식

HRID 1252794 반응식
OS(O)(=O)=O.O[C:7]1[CH2:12][CH2:11][CH2:10][C:9](=[O:13])[C:8]=1[CH2:14][C:15](=[O:17])[CH3:16]>C(Cl)Cl>[CH3:16][C:15]1[O:17][C:7]2[CH2:12][CH2:11][CH2:10][C:9](=[O:13])[C:8]=2[CH:14]=1

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 74817023-Hydroxy-2-(2-oxopropyl)-2-cyclohexen-1-one

생성물 1

HCID 64216646,7-Dihydro-2-methyl-4(5H) benzofuranone

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of conc. H2SO4 (300 ml) cooled in an ice-bath was added a solution of 3-hydroxy-2(2-oxopropyl)-2-cyclohexene-1-one (190 g in 300 ml CH2Cl2). Upon completion of addition, the mixture was stirred at ambient temperature for about 1 hour. The mixture was then slowly poured into 3 l ice water, and then about 1 l of CH2Cl2 was added. The layers are separated and the aqueous layer extracted thrice with CH2Cl2 and the combined CH2Cl2 layers again extracted thrice with water. The CH2Cl2 layer washed thrice with dilute aqueous NaHCO3, then once with water and dried (MgSO4). Concentration in vacuo afford an orange oil.

후처리

  1. additionUpon completion of addition
  2. customThe layers are separated
  3. extractionthe aqueous layer extracted thrice with CH2Cl2
  4. washThe CH2Cl2 layer washed thrice with dilute aqueous NaHCO3
  5. dry with materialonce with water and dried (MgSO4)
  6. concentrationConcentration in vacuo
  7. customafford an orange oil

출처 및 근거

ORD 기록
ord-27938cde0583418c82206b978208bd88
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04745222

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